+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 14:33:49 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SOT096 P2(1)2(1)2(1) CELL 0.71073 11.4829 14.5419 15.7595 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0003 0.0004 0.000 0.000 0.000 LATT -1 SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 - X, - Y, 1/2 + Z SFAC C H N O SI UNIT 108 144 8 24 4 V = 2631.57 F(000) = 1096.0 Mu = 0.13 mm-1 Cell Wt = 2050.67 Rho = 1.294 MERG 2 SHEL 7 0.84 FMAP 2 TWIN BASF 0.2 PLAN 10 L.S. 4 TEMP -153.00 WGHT 0.043500 EXTI 0.005193 FVAR 0.31169 C1 1 0.245989 0.307460 0.550083 11.00000 0.02373 0.01165 = 0.01813 -0.00156 0.00710 0.00250 C2 1 0.316752 0.372243 0.587298 11.00000 0.02294 0.02068 = 0.01939 0.00016 -0.00091 0.00083 AFIX 43 H2 2 0.384026 0.354247 0.618205 11.00000 -1.20000 AFIX 0 C3 1 0.287759 0.464702 0.578739 11.00000 0.02181 0.01716 = 0.02173 -0.00110 -0.00061 -0.00097 AFIX 43 H3 2 0.335639 0.510415 0.603987 11.00000 -1.20000 AFIX 0 C4 1 0.188845 0.490649 0.533323 11.00000 0.02249 0.01665 = 0.01218 0.00120 0.00413 -0.00090 C5 1 0.118860 0.422768 0.497087 11.00000 0.02178 0.02229 = 0.01759 0.00024 -0.00033 0.00028 AFIX 43 H5 2 0.051159 0.440011 0.466309 11.00000 -1.20000 AFIX 0 C6 1 0.146896 0.330315 0.505433 11.00000 0.02186 0.01887 = 0.02135 -0.00561 0.00465 -0.00539 AFIX 43 H6 2 0.099056 0.284046 0.481021 11.00000 -1.20000 AFIX 0 C7 1 0.156324 0.590529 0.522275 11.00000 0.01809 0.01799 = 0.01368 -0.00050 0.00010 -0.00186 AFIX 13 H7 2 0.138575 0.602698 0.461176 11.00000 -1.20000 AFIX 0 C8 1 0.053872 0.623500 0.577287 11.00000 0.01715 0.01817 = 0.01577 -0.00208 0.00214 -0.00249 AFIX 23 H8A 2 0.049185 0.587379 0.630426 11.00000 -1.20000 H8B 2 -0.020622 0.617150 0.546212 11.00000 -1.20000 AFIX 0 C9 1 0.079802 0.726324 0.596826 11.00000 0.01453 0.01701 = 0.01620 0.00049 -0.00050 0.00017 C10 1 0.016331 0.790993 0.533878 11.00000 0.01937 0.02000 = 0.01564 -0.00109 -0.00266 0.00075 AFIX 23 H10A 2 -0.060448 0.765590 0.517534 11.00000 -1.20000 H10B 2 0.005074 0.852854 0.558790 11.00000 -1.20000 AFIX 0 C11 1 0.098096 0.794803 0.458074 11.00000 0.01937 0.01487 = 0.01778 -0.00030 -0.00032 0.00138 AFIX 13 H11 2 0.088704 0.737641 0.423468 11.00000 -1.20000 AFIX 0 C12 1 0.209082 0.736028 0.568525 11.00000 0.02079 0.01408 = 0.01622 0.00002 0.00200 0.00070 AFIX 13 H12 2 0.256126 0.763284 0.615630 11.00000 -1.20000 AFIX 0 C13 1 0.084071 0.877869 0.401521 11.00000 0.01686 0.01432 = 0.01786 0.00112 0.00306 0.00298 C14 1 0.122794 0.964583 0.425873 11.00000 0.02368 0.01926 = 0.01978 0.00099 -0.00213 -0.00221 AFIX 43 H14 2 0.159482 0.972647 0.479387 11.00000 -1.20000 AFIX 0 C15 1 0.108022 1.039157 0.372353 11.00000 0.02352 0.01673 = 0.03187 0.00093 -0.00423 -0.00275 AFIX 43 H15 2 0.133905 1.098645 0.388630 11.00000 -1.20000 AFIX 0 C16 1 0.054944 1.025279 0.294913 11.00000 0.01636 0.02060 = 0.02842 0.00929 0.00338 0.00288 C17 1 0.014782 0.940391 0.269146 11.00000 0.02113 0.02452 = 0.01758 0.00163 -0.00167 0.00168 AFIX 43 H17 2 -0.021560 0.932528 0.215481 11.00000 -1.20000 AFIX 0 C18 1 0.029179 0.867142 0.324015 11.00000 0.02090 0.01877 = 0.02234 -0.00208 -0.00177 -0.00190 AFIX 43 H18 2 0.000802 0.808223 0.308186 11.00000 -1.20000 AFIX 0 C19 1 0.097226 0.660335 0.782712 11.00000 0.02369 0.02393 = 0.01642 -0.00120 -0.00345 -0.00216 AFIX 13 H19 2 0.053608 0.605504 0.761345 11.00000 -1.20000 AFIX 0 C20 1 0.064890 0.670350 0.876822 11.00000 0.03660 0.04809 = 0.01946 0.00725 0.00045 0.00867 AFIX 33 H20A 2 -0.017978 0.685539 0.881794 11.00000 -1.50000 H20B 2 0.111534 0.719546 0.902338 11.00000 -1.50000 H20C 2 0.080480 0.612353 0.906386 11.00000 -1.50000 AFIX 0 C21 1 0.226691 0.636570 0.775026 11.00000 0.02584 0.02629 = 0.02771 0.00676 -0.00245 0.00232 AFIX 33 H21A 2 0.247035 0.628937 0.715046 11.00000 -1.50000 H21B 2 0.242523 0.579221 0.805581 11.00000 -1.50000 H21C 2 0.273382 0.686339 0.799531 11.00000 -1.50000 AFIX 0 C22 1 -0.107756 0.782665 0.734253 11.00000 0.01837 0.03121 = 0.01576 -0.00361 0.00000 0.00424 AFIX 13 H22 2 -0.112487 0.797735 0.796069 11.00000 -1.20000 AFIX 0 C23 1 -0.181774 0.696336 0.723075 11.00000 0.02080 0.04106 = 0.02879 -0.00072 -0.00022 -0.00488 AFIX 33 H23A 2 -0.144432 0.644628 0.752232 11.00000 -1.50000 H23B 2 -0.189157 0.682183 0.662516 11.00000 -1.50000 H23C 2 -0.259258 0.706766 0.747300 11.00000 -1.50000 AFIX 0 C24 1 -0.164634 0.864697 0.688616 11.00000 0.02211 0.04381 = 0.02830 -0.00119 0.00094 0.01299 AFIX 33 H24A 2 -0.116428 0.919651 0.696485 11.00000 -1.50000 H24B 2 -0.242280 0.875623 0.712375 11.00000 -1.50000 H24C 2 -0.171425 0.851072 0.627917 11.00000 -1.50000 AFIX 0 C25 1 0.140710 0.866163 0.743270 11.00000 0.01873 0.02335 = 0.02086 -0.00473 -0.00198 0.00132 AFIX 13 H25 2 0.219573 0.842912 0.759524 11.00000 -1.20000 AFIX 0 C26 1 0.091401 0.913488 0.822775 11.00000 0.03673 0.03220 = 0.02732 -0.01185 -0.00182 0.00177 AFIX 33 H26A 2 0.078443 0.867510 0.867248 11.00000 -1.50000 H26B 2 0.017415 0.943410 0.808685 11.00000 -1.50000 H26C 2 0.146917 0.959709 0.843066 11.00000 -1.50000 AFIX 0 C27 1 0.161218 0.939390 0.674410 11.00000 0.03116 0.01996 = 0.03071 -0.00337 -0.00253 -0.00255 AFIX 33 H27A 2 0.193200 0.910046 0.623511 11.00000 -1.50000 H27B 2 0.216330 0.985499 0.695486 11.00000 -1.50000 H27C 2 0.087186 0.969269 0.660371 11.00000 -1.50000 AFIX 0 N1 3 0.280870 0.209742 0.556156 11.00000 0.02868 0.01867 = 0.02393 -0.00054 0.00562 0.00165 N2 3 0.040410 1.104054 0.237798 11.00000 0.01869 0.02946 = 0.04360 0.01881 -0.00317 -0.00026 O1 4 0.374317 0.191311 0.589715 11.00000 0.03202 0.02332 = 0.05025 0.00296 -0.00239 0.00697 O2 4 0.214746 0.151456 0.526972 11.00000 0.04513 0.01733 = 0.05006 -0.00902 -0.00428 -0.00442 O3 4 0.059827 1.181188 0.266472 11.00000 0.04461 0.02247 = 0.06830 0.01906 -0.01773 -0.00677 O4 4 0.009703 1.089869 0.164469 11.00000 0.05606 0.04883 = 0.03618 0.02467 -0.01378 0.00117 O5 4 0.251994 0.647267 0.548503 11.00000 0.01602 0.01422 = 0.02320 -0.00023 0.00221 0.00037 O6 4 0.211979 0.795327 0.496543 11.00000 0.01705 0.01675 = 0.01917 0.00532 0.00193 -0.00059 SI1 5 0.051899 0.760474 0.713016 11.00000 0.01567 0.02014 = 0.01414 -0.00160 -0.00025 0.00084 HKLF 4 Covalent radii and connectivity table for 01SOT096 P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 C1 - C2 C6 N1 C2 - C1 C3 C3 - C2 C4 C4 - C3 C5 C7 C5 - C6 C4 C6 - C1 C5 C7 - O5 C4 C8 C8 - C7 C9 C9 - C10 C8 C12 Si1 C10 - C11 C9 C11 - O6 C13 C10 C12 - O5 O6 C9 C13 - C18 C14 C11 C14 - C15 C13 C15 - C16 C14 C16 - C17 C15 N2 C17 - C16 C18 C18 - C17 C13 C19 - C21 C20 Si1 C20 - C19 C21 - C19 C22 - C23 C24 Si1 C23 - C22 C24 - C22 C25 - C26 C27 Si1 C26 - C25 C27 - C25 N1 - O1 O2 C1 N2 - O4 O3 C16 O1 - N1 O2 - N1 O3 - N2 O4 - N2 O5 - C12 C7 O6 - C12 C11 Si1 - C22 C19 C25 C9 3324 Reflections read, of which 700 rejected 0 =< h =< 13, 0 =< k =< 17, 0 =< l =< 18, Max. 2-theta = 50.04 0 Systematic absence violations 0 Inconsistent equivalents 2624 Unique reflections, of which 0 suppressed R(int) = 0.0000 R(sigma) = 0.0463 Friedel opposites not merged Maximum memory for data reduction = 2810 / 25587 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 3785 / 412493 wR2 = 0.0739 before cycle 1 for 2624 data and 327 / 327 parameters GooF = S = 1.007; Restrained GooF = 1.007 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0435 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31163 0.00058 -0.106 OSF 2 0.44158 0.15477 1.561 BASF 1 3 0.00515 0.00091 -0.050 EXTI Mean shift/esd = 0.049 Maximum = 1.561 for BASF 1 Max. shift = 0.000 A for C22 Max. dU = 0.000 for C26 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3785 / 412493 wR2 = 0.0738 before cycle 2 for 2624 data and 327 / 327 parameters GooF = S = 1.005; Restrained GooF = 1.005 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0435 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31161 0.00058 -0.031 OSF 2 0.52322 0.15465 0.528 BASF 1 3 0.00513 0.00091 -0.018 EXTI Mean shift/esd = 0.017 Maximum = 0.528 for BASF 1 Max. shift = 0.000 A for C22 Max. dU = 0.000 for C26 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3785 / 412493 wR2 = 0.0738 before cycle 3 for 2624 data and 327 / 327 parameters GooF = S = 1.005; Restrained GooF = 1.005 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0435 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31161 0.00058 0.000 OSF 2 0.52394 0.15462 0.005 BASF 1 3 0.00513 0.00091 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.007 for U23 Si1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C27 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3785 / 412493 wR2 = 0.0738 before cycle 4 for 2624 data and 327 / 327 parameters GooF = S = 1.005; Restrained GooF = 1.005 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0435 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31161 0.00058 0.000 OSF 2 0.52404 0.15463 0.001 BASF 1 3 0.00513 0.00091 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for y C1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C22 Largest correlation matrix elements 0.500 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3840 0.3542 0.6182 43 0.950 0.000 C2 C1 C3 H3 0.3357 0.5104 0.6040 43 0.950 0.000 C3 C2 C4 H5 0.0511 0.4400 0.4663 43 0.950 0.000 C5 C6 C4 H6 0.0991 0.2840 0.4810 43 0.950 0.000 C6 C1 C5 H7 0.1385 0.6027 0.4612 13 1.000 0.000 C7 O5 C4 C8 H8A 0.0492 0.5874 0.6304 23 0.990 0.000 C8 C7 C9 H8B -0.0206 0.6171 0.5462 23 0.990 0.000 C8 C7 C9 H10A -0.0604 0.7656 0.5175 23 0.990 0.000 C10 C11 C9 H10B 0.0051 0.8529 0.5588 23 0.990 0.000 C10 C11 C9 H11 0.0887 0.7376 0.4235 13 1.000 0.000 C11 O6 C13 C10 H12 0.2561 0.7633 0.6156 13 1.000 0.000 C12 O5 O6 C9 H14 0.1595 0.9726 0.4794 43 0.950 0.000 C14 C15 C13 H15 0.1339 1.0987 0.3887 43 0.950 0.000 C15 C16 C14 H17 -0.0215 0.9325 0.2155 43 0.950 0.000 C17 C16 C18 H18 0.0008 0.8082 0.3082 43 0.950 0.000 C18 C17 C13 H19 0.0536 0.6055 0.7614 13 1.000 0.000 C19 C21 C20 Si1 H20A -0.0180 0.6855 0.8818 33 0.980 0.000 C20 C19 H20A H20B 0.1115 0.7195 0.9024 33 0.980 0.000 C20 C19 H20A H20C 0.0805 0.6123 0.9064 33 0.980 0.000 C20 C19 H20A H21A 0.2470 0.6289 0.7150 33 0.980 0.000 C21 C19 H21A H21B 0.2426 0.5792 0.8056 33 0.980 0.000 C21 C19 H21A H21C 0.2734 0.6863 0.7995 33 0.980 0.000 C21 C19 H21A H22 -0.1125 0.7978 0.7961 13 1.000 0.000 C22 C23 C24 Si1 H23A -0.1444 0.6446 0.7522 33 0.980 0.000 C23 C22 H23A H23B -0.1891 0.6822 0.6625 33 0.980 0.000 C23 C22 H23A H23C -0.2593 0.7068 0.7473 33 0.980 0.000 C23 C22 H23A H24A -0.1165 0.9197 0.6965 33 0.980 0.000 C24 C22 H24A H24B -0.2423 0.8756 0.7124 33 0.980 0.000 C24 C22 H24A H24C -0.1714 0.8510 0.6279 33 0.980 0.000 C24 C22 H24A H25 0.2196 0.8429 0.7595 13 1.000 0.000 C25 C26 C27 Si1 H26A 0.0785 0.8675 0.8672 33 0.980 0.000 C26 C25 H26A H26B 0.0174 0.9434 0.8087 33 0.980 0.000 C26 C25 H26A H26C 0.1469 0.9597 0.8431 33 0.980 0.000 C26 C25 H26A H27A 0.1932 0.9100 0.6235 33 0.980 0.000 C27 C25 H27A H27B 0.2163 0.9855 0.6955 33 0.980 0.000 C27 C25 H27A H27C 0.0872 0.9693 0.6604 33 0.980 0.000 C27 C25 H27A 01SOT096 P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.24597 0.30747 0.55008 1.00000 0.02369 0.01165 0.01808 -0.00167 0.00717 0.00236 0.01781 0.00425 0.00022 0.00015 0.00015 0.00000 0.00134 0.00106 0.00116 0.00105 0.00115 0.00105 0.00053 C2 0.31676 0.37223 0.58729 1.00000 0.02298 0.02061 0.01925 0.00025 -0.00095 0.00087 0.02095 0.00412 0.00021 0.00016 0.00015 0.00000 0.00139 0.00129 0.00119 0.00117 0.00113 0.00110 0.00056 H2 0.38404 0.35423 0.61819 1.00000 0.02513 0.00000 0.00000 C3 0.28777 0.46470 0.57872 1.00000 0.02185 0.01722 0.02169 -0.00108 -0.00062 -0.00109 0.02025 0.00430 0.00021 0.00016 0.00015 0.00000 0.00134 0.00121 0.00128 0.00110 0.00111 0.00105 0.00055 H3 0.33565 0.51042 0.60396 1.00000 0.02430 0.00000 0.00000 C4 0.18885 0.49063 0.53331 1.00000 0.02244 0.01675 0.01211 0.00125 0.00410 -0.00095 0.01710 0.00401 0.00021 0.00015 0.00014 0.00000 0.00134 0.00119 0.00111 0.00105 0.00106 0.00104 0.00053 C5 0.11884 0.42277 0.49706 1.00000 0.02183 0.02227 0.01751 0.00028 -0.00031 0.00031 0.02054 0.00405 0.00022 0.00016 0.00014 0.00000 0.00135 0.00123 0.00114 0.00109 0.00115 0.00105 0.00054 H5 0.05115 0.44002 0.46627 1.00000 0.02464 0.00000 0.00000 C6 0.14690 0.33031 0.50542 1.00000 0.02179 0.01882 0.02130 -0.00562 0.00453 -0.00531 0.02064 0.00423 0.00022 0.00016 0.00015 0.00000 0.00137 0.00121 0.00127 0.00111 0.00115 0.00106 0.00056 H6 0.09907 0.28403 0.48101 1.00000 0.02476 0.00000 0.00000 C7 0.15629 0.59052 0.52227 1.00000 0.01803 0.01791 0.01367 -0.00051 0.00022 -0.00190 0.01654 0.00382 0.00020 0.00015 0.00014 0.00000 0.00126 0.00116 0.00112 0.00103 0.00105 0.00104 0.00052 H7 0.13854 0.60269 0.46117 1.00000 0.01984 0.00000 0.00000 C8 0.05387 0.62350 0.57728 1.00000 0.01724 0.01822 0.01576 -0.00208 0.00219 -0.00246 0.01708 0.00399 0.00021 0.00015 0.00014 0.00000 0.00125 0.00115 0.00112 0.00103 0.00107 0.00104 0.00051 H8A 0.04919 0.58738 0.63042 1.00000 0.02049 0.00000 0.00000 H8B -0.02063 0.61714 0.54621 1.00000 0.02049 0.00000 0.00000 C9 0.07978 0.72631 0.59681 1.00000 0.01470 0.01704 0.01604 0.00045 -0.00044 0.00017 0.01593 0.00384 0.00019 0.00015 0.00014 0.00000 0.00121 0.00118 0.00107 0.00104 0.00097 0.00093 0.00051 C10 0.01634 0.79099 0.53388 1.00000 0.01934 0.02020 0.01546 -0.00098 -0.00269 0.00069 0.01833 0.00393 0.00020 0.00016 0.00014 0.00000 0.00128 0.00119 0.00114 0.00106 0.00104 0.00101 0.00054 H10A -0.06045 0.76561 0.51753 1.00000 0.02200 0.00000 0.00000 H10B 0.00511 0.85285 0.55879 1.00000 0.02200 0.00000 0.00000 C11 0.09809 0.79479 0.45808 1.00000 0.01926 0.01493 0.01779 -0.00030 -0.00032 0.00144 0.01733 0.00408 0.00020 0.00016 0.00015 0.00000 0.00128 0.00116 0.00117 0.00107 0.00107 0.00100 0.00053 H11 0.08869 0.73763 0.42347 1.00000 0.02079 0.00000 0.00000 C12 0.20909 0.73604 0.56853 1.00000 0.02090 0.01409 0.01617 0.00019 0.00201 0.00064 0.01705 0.00416 0.00021 0.00016 0.00014 0.00000 0.00130 0.00114 0.00117 0.00104 0.00101 0.00102 0.00053 H12 0.25612 0.76330 0.61563 1.00000 0.02046 0.00000 0.00000 C13 0.08408 0.87788 0.40152 1.00000 0.01676 0.01419 0.01791 0.00114 0.00301 0.00289 0.01629 0.00399 0.00020 0.00015 0.00014 0.00000 0.00128 0.00118 0.00117 0.00106 0.00102 0.00097 0.00053 C14 0.12279 0.96459 0.42589 1.00000 0.02382 0.01917 0.01973 0.00100 -0.00218 -0.00207 0.02090 0.00413 0.00022 0.00016 0.00015 0.00000 0.00138 0.00126 0.00124 0.00108 0.00111 0.00111 0.00056 H14 0.15947 0.97265 0.47941 1.00000 0.02509 0.00000 0.00000 C15 0.10800 1.03916 0.37237 1.00000 0.02346 0.01667 0.03192 0.00090 -0.00441 -0.00272 0.02402 0.00431 0.00021 0.00016 0.00017 0.00000 0.00137 0.00122 0.00139 0.00118 0.00120 0.00113 0.00058 H15 0.13386 1.09865 0.38865 1.00000 0.02882 0.00000 0.00000 C16 0.05493 1.02526 0.29490 1.00000 0.01639 0.02064 0.02821 0.00932 0.00337 0.00280 0.02175 0.00430 0.00021 0.00016 0.00015 0.00000 0.00123 0.00121 0.00136 0.00118 0.00120 0.00107 0.00055 C17 0.01479 0.94039 0.26914 1.00000 0.02104 0.02449 0.01763 0.00166 -0.00167 0.00157 0.02105 0.00414 0.00021 0.00015 0.00015 0.00000 0.00138 0.00130 0.00124 0.00111 0.00113 0.00104 0.00057 H17 -0.02154 0.93253 0.21547 1.00000 0.02526 0.00000 0.00000 C18 0.02917 0.86713 0.32403 1.00000 0.02095 0.01876 0.02230 -0.00195 -0.00174 -0.00201 0.02067 0.00411 0.00021 0.00016 0.00015 0.00000 0.00134 0.00121 0.00124 0.00114 0.00114 0.00108 0.00055 H18 0.00079 0.80821 0.30822 1.00000 0.02480 0.00000 0.00000 C19 0.09725 0.66032 0.78274 1.00000 0.02353 0.02383 0.01640 -0.00113 -0.00354 -0.00217 0.02125 0.00410 0.00022 0.00016 0.00015 0.00000 0.00133 0.00125 0.00120 0.00114 0.00110 0.00107 0.00056 H19 0.05363 0.60549 0.76137 1.00000 0.02550 0.00000 0.00000 C20 0.06487 0.67034 0.87682 1.00000 0.03646 0.04817 0.01938 0.00735 0.00038 0.00877 0.03467 0.00508 0.00026 0.00020 0.00016 0.00000 0.00167 0.00173 0.00128 0.00127 0.00127 0.00144 0.00070 H20A -0.01800 0.68552 0.88177 1.00000 0.05200 0.00000 0.00000 H20B 0.11150 0.71953 0.90235 1.00000 0.05200 0.00000 0.00000 H20C 0.08045 0.61234 0.90639 1.00000 0.05200 0.00000 0.00000 C21 0.22671 0.63656 0.77502 1.00000 0.02587 0.02625 0.02760 0.00670 -0.00243 0.00233 0.02657 0.00460 0.00022 0.00018 0.00017 0.00000 0.00146 0.00125 0.00141 0.00126 0.00124 0.00117 0.00060 H21A 0.24702 0.62893 0.71503 1.00000 0.03986 0.00000 0.00000 H21B 0.24255 0.57921 0.80556 1.00000 0.03986 0.00000 0.00000 H21C 0.27341 0.68633 0.79951 1.00000 0.03986 0.00000 0.00000 C22 -0.10774 0.78269 0.73428 1.00000 0.01836 0.03102 0.01561 -0.00344 0.00008 0.00437 0.02167 0.00418 0.00021 0.00016 0.00015 0.00000 0.00127 0.00135 0.00114 0.00109 0.00107 0.00108 0.00056 H22 -0.11247 0.79776 0.79610 1.00000 0.02600 0.00000 0.00000 C23 -0.18177 0.69634 0.72308 1.00000 0.02071 0.04106 0.02881 -0.00091 -0.00032 -0.00490 0.03019 0.00436 0.00022 0.00018 0.00017 0.00000 0.00141 0.00152 0.00144 0.00134 0.00124 0.00123 0.00063 H23A -0.14443 0.64463 0.75224 1.00000 0.04529 0.00000 0.00000 H23B -0.18914 0.68219 0.66252 1.00000 0.04529 0.00000 0.00000 H23C -0.25926 0.70676 0.74730 1.00000 0.04529 0.00000 0.00000 C24 -0.16466 0.86469 0.68863 1.00000 0.02212 0.04373 0.02834 -0.00112 0.00115 0.01282 0.03140 0.00490 0.00023 0.00019 0.00017 0.00000 0.00142 0.00160 0.00147 0.00136 0.00123 0.00131 0.00066 H24A -0.11648 0.91966 0.69648 1.00000 0.04709 0.00000 0.00000 H24B -0.24231 0.87560 0.71239 1.00000 0.04709 0.00000 0.00000 H24C -0.17145 0.85104 0.62793 1.00000 0.04709 0.00000 0.00000 C25 0.14071 0.86618 0.74326 1.00000 0.01869 0.02339 0.02103 -0.00487 -0.00223 0.00119 0.02104 0.00403 0.00021 0.00016 0.00015 0.00000 0.00133 0.00123 0.00123 0.00112 0.00109 0.00107 0.00055 H25 0.21957 0.84293 0.75951 1.00000 0.02525 0.00000 0.00000 C26 0.09141 0.91351 0.82277 1.00000 0.03698 0.03224 0.02743 -0.01191 -0.00184 0.00183 0.03221 0.00455 0.00025 0.00018 0.00016 0.00000 0.00168 0.00150 0.00133 0.00127 0.00134 0.00131 0.00067 H26A 0.07845 0.86753 0.86724 1.00000 0.04832 0.00000 0.00000 H26B 0.01742 0.94343 0.80869 1.00000 0.04832 0.00000 0.00000 H26C 0.14693 0.95972 0.84306 1.00000 0.04832 0.00000 0.00000 C27 0.16121 0.93938 0.67442 1.00000 0.03118 0.01996 0.03067 -0.00342 -0.00257 -0.00255 0.02727 0.00433 0.00023 0.00016 0.00017 0.00000 0.00153 0.00129 0.00140 0.00122 0.00130 0.00116 0.00062 H27A 0.19319 0.91003 0.62352 1.00000 0.04090 0.00000 0.00000 H27B 0.21632 0.98549 0.69550 1.00000 0.04090 0.00000 0.00000 H27C 0.08718 0.96926 0.66038 1.00000 0.04090 0.00000 0.00000 N1 0.28085 0.20975 0.55615 1.00000 0.02866 0.01869 0.02392 -0.00053 0.00557 0.00173 0.02376 0.00388 0.00020 0.00014 0.00013 0.00000 0.00133 0.00111 0.00111 0.00096 0.00103 0.00101 0.00051 N2 0.04043 1.10405 0.23782 1.00000 0.01859 0.02943 0.04370 0.01883 -0.00325 -0.00021 0.03058 0.00422 0.00019 0.00015 0.00016 0.00000 0.00121 0.00129 0.00142 0.00115 0.00116 0.00101 0.00055 O1 0.37434 0.19132 0.58972 1.00000 0.03198 0.02323 0.05042 0.00296 -0.00235 0.00687 0.03521 0.00336 0.00017 0.00012 0.00013 0.00000 0.00114 0.00092 0.00118 0.00097 0.00103 0.00087 0.00047 O2 0.21475 0.15145 0.52698 1.00000 0.04506 0.01737 0.05011 -0.00904 -0.00429 -0.00447 0.03751 0.00331 0.00017 0.00012 0.00013 0.00000 0.00123 0.00088 0.00126 0.00095 0.00107 0.00091 0.00052 O3 0.05984 1.18117 0.26648 1.00000 0.04465 0.02252 0.06843 0.01914 -0.01766 -0.00675 0.04520 0.00348 0.00018 0.00012 0.00014 0.00000 0.00126 0.00099 0.00144 0.00108 0.00121 0.00092 0.00057 O4 0.00969 1.08988 0.16448 1.00000 0.05601 0.04884 0.03607 0.02470 -0.01371 0.00106 0.04697 0.00378 0.00019 0.00014 0.00013 0.00000 0.00142 0.00130 0.00118 0.00108 0.00115 0.00109 0.00059 O5 0.25199 0.64726 0.54850 1.00000 0.01606 0.01422 0.02310 -0.00027 0.00217 0.00038 0.01779 0.00273 0.00014 0.00010 0.00010 0.00000 0.00086 0.00076 0.00087 0.00073 0.00075 0.00071 0.00037 O6 0.21196 0.79532 0.49653 1.00000 0.01706 0.01666 0.01913 0.00540 0.00192 -0.00060 0.01762 0.00270 0.00013 0.00010 0.00010 0.00000 0.00088 0.00080 0.00083 0.00072 0.00075 0.00069 0.00038 Si1 0.05191 0.76047 0.71302 1.00000 0.01564 0.02014 0.01415 -0.00160 -0.00020 0.00081 0.01664 0.00107 0.00006 0.00004 0.00004 0.00000 0.00034 0.00033 0.00031 0.00029 0.00027 0.00028 0.00017 Final Structure Factor Calculation for 01SOT096 P2(1)2(1)2(1) Total number of l.s. parameters = 327 Maximum vector length = 511 Memory required = 3460 / 26068 wR2 = 0.0738 before cycle 5 for 2624 data and 2 / 327 parameters GooF = S = 1.005; Restrained GooF = 1.005 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0435 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0307 for 2328 Fo > 4sig(Fo) and 0.0363 for all 2624 data wR2 = 0.0738, GooF = S = 1.005, Restrained GooF = 1.005 for all data Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 36.00 for hydrogen atoms Principal mean square atomic displacements U 0.0286 0.0152 0.0096 C1 0.0234 0.0205 0.0189 C2 0.0224 0.0217 0.0167 C3 0.0239 0.0171 0.0103 C4 0.0224 0.0217 0.0175 C5 0.0310 0.0170 0.0139 C6 0.0199 0.0161 0.0136 C7 0.0218 0.0153 0.0142 C8 0.0172 0.0160 0.0145 C9 0.0216 0.0194 0.0140 C10 0.0198 0.0177 0.0145 C11 0.0217 0.0154 0.0140 C12 0.0215 0.0152 0.0122 C13 0.0256 0.0188 0.0183 C14 0.0340 0.0223 0.0157 C15 0.0355 0.0156 0.0142 C16 0.0252 0.0215 0.0164 C17 0.0236 0.0220 0.0164 C18 0.0262 0.0230 0.0146 C19 0.0542 0.0324 0.0174 C20 0.0337 0.0274 0.0186 C21 0.0330 0.0175 0.0145 C22 0.0422 0.0288 0.0196 C23 0.0497 0.0285 0.0160 C24 0.0278 0.0187 0.0166 C25 0.0431 0.0359 0.0177 C26 0.0335 0.0301 0.0182 C27 0.0324 0.0210 0.0178 N1 0.0569 0.0193 0.0155 N2 0.0509 0.0357 0.0190 O1 0.0536 0.0448 0.0141 O2 0.0844 0.0357 0.0156 O3 0.0721 0.0550 0.0137 O4 0.0237 0.0156 0.0141 O5 0.0236 0.0174 0.0118 O6 0.0207 0.0155 0.0137 Si1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.028 0.043 0.057 0.071 0.084 0.102 0.120 0.150 0.200 1.000 Number in group 272. 264. 258. 266. 261. 262. 255. 266. 258. 262. GooF 0.725 1.018 0.906 1.037 1.023 1.042 1.150 1.100 0.941 1.053 K 1.268 0.998 1.010 0.983 1.001 0.998 0.999 1.006 1.013 1.014 Resolution(A) 0.84 0.87 0.91 0.95 1.01 1.07 1.15 1.28 1.47 1.87 inf Number in group 268. 264. 260. 273. 247. 268. 255. 263. 263. 263. GooF 0.753 0.756 0.809 0.891 0.933 0.902 1.008 0.979 1.281 1.491 K 1.028 1.030 1.018 1.007 1.007 1.008 1.006 1.009 1.029 1.003 R1 0.088 0.063 0.054 0.047 0.038 0.029 0.027 0.026 0.028 0.024 Recommended weighting scheme: WGHT 0.0415 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 0 8 4 185.22 126.95 5.39 0.062 1.65 0 6 4 396.21 312.73 4.94 0.097 2.06 4 0 5 800.84 660.99 4.05 0.141 2.12 2 4 0 41.20 27.60 4.04 0.029 3.07 1 7 2 60.77 42.14 3.97 0.036 1.98 10 5 10 0.00 3.68 3.78 0.011 0.88 3 8 8 369.80 463.67 3.78 0.118 1.26 2 7 1 62.83 82.75 3.77 0.050 1.94 4 3 4 393.81 472.20 3.70 0.119 2.09 4 1 3 22.25 36.96 3.52 0.033 2.48 2 3 4 66.45 84.33 3.50 0.050 2.70 7 0 16 135.77 236.63 3.44 0.084 0.84 2 5 2 592.72 504.45 3.35 0.123 2.46 0 13 7 221.77 138.34 3.31 0.065 1.00 2 2 0 484.81 565.70 3.30 0.131 4.51 0 10 10 84.26 148.05 3.18 0.067 1.07 7 0 12 1.03 13.30 3.15 0.020 1.03 5 5 0 30.79 16.29 3.07 0.022 1.80 4 5 1 446.38 382.38 3.06 0.107 2.03 5 2 1 81.38 101.62 3.03 0.055 2.17 3 5 2 1314.76 1146.62 3.01 0.186 2.22 4 0 1 250.45 216.07 3.00 0.081 2.82 5 0 1 745.50 646.00 3.00 0.139 2.27 4 7 4 61.28 44.62 2.97 0.037 1.55 3 10 6 313.99 375.34 2.94 0.106 1.21 1 15 3 100.22 139.83 2.89 0.065 0.95 0 5 2 43.26 53.01 2.81 0.040 2.73 7 2 7 146.39 182.60 2.79 0.074 1.30 2 3 8 51.70 37.82 2.75 0.034 1.74 12 4 0 885.76 707.11 2.73 0.146 0.93 0 6 6 389.90 445.76 2.72 0.116 1.78 8 1 0 684.81 595.98 2.71 0.134 1.43 0 9 2 372.24 327.46 2.66 0.099 1.58 3 7 0 673.35 589.60 2.66 0.133 1.83 0 6 1 471.26 416.45 2.66 0.112 2.40 2 1 9 138.76 115.87 2.63 0.059 1.66 1 1 5 665.99 754.16 2.63 0.151 2.98 3 5 6 125.48 147.48 2.63 0.067 1.74 2 7 6 434.11 376.14 2.62 0.106 1.57 4 5 4 719.41 812.73 2.60 0.156 1.81 0 4 10 280.81 324.54 2.59 0.099 1.45 3 12 0 1278.04 1125.17 2.58 0.184 1.16 1 2 10 804.13 707.51 2.57 0.146 1.53 3 8 0 27.71 40.45 2.56 0.035 1.64 0 6 5 45.42 37.12 2.55 0.033 1.92 1 7 3 2520.36 2246.85 2.55 0.260 1.91 2 5 0 494.13 557.24 2.52 0.130 2.59 1 6 6 296.06 259.60 2.52 0.088 1.76 1 4 3 1021.90 1149.62 2.51 0.186 2.89 2 3 7 483.88 549.23 2.51 0.129 1.92 FMAP and GRID set by program FMAP 2 3 19 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0362 for 2624 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.2058 0.2459 0.0949 [ 0.56 A from H12 ] Deepest hole -0.20 at 0.4850 0.2865 0.2116 [ 0.80 A from SI1 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 3317 / 22893 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2942 0.7541 0.5949 1.00000 0.05 0.29 0.56 H12 1.09 C12 1.78 O5 1.91 O6 Q2 1 -0.0368 0.7664 0.7213 1.00000 0.05 0.21 0.87 C22 1.03 SI1 1.53 H22 1.95 C23 Q3 1 0.0847 0.6327 0.7695 1.00000 0.05 0.17 0.48 C19 0.55 H19 1.63 C21 1.79 C20 Q4 1 0.1326 0.7260 0.5900 1.00000 0.05 0.15 0.62 C9 0.95 C12 1.57 H12 1.75 C8 Q5 1 0.0502 0.7501 0.5749 1.00000 0.05 0.15 0.60 C9 0.96 C10 1.58 H10A 1.60 H10B Q6 1 0.0916 0.8413 0.4259 1.00000 0.05 0.15 0.66 C13 0.85 C11 1.51 H11 1.80 C18 Q7 1 0.0646 0.6824 0.5998 1.00000 0.05 0.14 0.66 C9 0.94 C8 1.47 H8A 1.60 H8B Q8 1 -0.2797 0.7241 0.7222 1.00000 0.05 0.14 0.52 H23C 1.19 C23 1.53 H23B 1.99 H23A Q9 1 0.2417 0.9050 0.4673 1.00000 0.05 0.14 1.38 H14 1.70 O6 1.74 C14 2.12 C13 Q10 1 0.0809 0.8421 0.7245 1.00000 0.05 0.14 0.82 C25 1.25 SI1 1.68 H25 1.86 C27 Shortest distances between peaks (including symmetry equivalents) 4 7 1.02 4 5 1.04 5 7 1.07 2 10 1.74 1 4 1.90 6 9 2.06 2 3 2.51 2 5 2.53 2 7 2.55 5 10 2.73 5 6 2.74 4 10 2.78 3 7 2.78 1 5 2.82 1 7 2.84 2 8 2.86 2 4 2.90 6 8 2.92 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 0.45: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 5.42: Structure factors and derivatives 2.11: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.66: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:34:00 Total CPU time: 9.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++